참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 5-Amino-2-(trifluoromethyl)pyridine | HCID 2737744 | — |
| 반응물 | 5-Bromo-2-fluoropyridine | HCID 2783168 | — |
| 용매 | 1-Butanol | HCID 263 | — |
| 생성물 | (5-Bromo-pyridin-2-yl)-(6-trifluoromethyl-pyridin-3-yl)-amine | HCID 66615754 | — |
반응 단계
A mixture of 5-amino-2-(trifluoromethyl)pyridine (0.5 g, 3.0 mmol, 1.0 equiv) and 5-bromo-2-fluoropyridine (0.47 mL, 4.6 mmol, 1.5 equiv) in 2 mL 1-butanol was charged with 0.15 mL of 4.0 M HCl (in dioxane) and heated to 150° C. via microwave heating. After cooling to room temperature, the reaction mixture was partitioned between ethyl acetate and saturated bicarbonate, and the organic extracts were washed with brine and dried over sodium sulphate. Purification of the crude product by flash chromatography afforded the title compound: 1H NMR (400 MHz, CDCl3) δ 6.63 (br. s., 1H) 6.67 (d, J=9.35 Hz, 1H) 7.56 (d, J=8.59 Hz, 1H) 7.62 (dd, J=8.84, 2.53 Hz, 1H) 8.22-8.66 (m, 2H) 8.57 (d, J=2.78 Hz, 1H); (M+H)+320.0.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08835451B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-1bb625d4c3f34e6aaf88132922120a2e |
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| 출처 메모 | uspto-grants-2014_09 |
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